Methods for synthesizing semiconductor quality chalcopyrite crystals for nonlinear optical and radiation detection applications and the like

Patent metadata

Field	Value
Publication number	US-9334581-B2
Application number	US-201213658591-A
Country	US
Kind code	B2
Filing date	Oct 23, 2012
Priority date	Oct 23, 2012
Publication date	May 10, 2016
Grant date	May 10, 2016

Abstract

A method for synthesizing I-III-VI 2 compounds, including: melting a Group III element; adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound; and adding a Group VI element to the single phase I-III compound under heat, with mixing, and/or via vapor transport. The Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C. Preferably, the Group I element consists of a neutron absorber and the group III element consists of In or Ga. The Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C. Preferably, the Group VI element consists of S, Se, or Te. Optionally, the method also includes doping with a Group IV element activator.

First claim

What is claimed is:

1. A method for synthesizing I-III-VI 2 compounds, comprising:
melting a Group III element;
subsequently adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound;
subsequently adding a Group VI element to the single phase I-III compound and heating; and
growing a bulk crystal from the resulting I-III-VI 2 compound without using a seed crystal.

2. The method of claim 1 , wherein the Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C.

3. The method of claim 1 , wherein 1 mole of the Group I element is added to 1 mole of the Group III element.

4. The method of claim 1 , wherein the Group I element comprises a neutron absorber and the Group III element comprises one of In and Ga.

5. The method of claim 1 , wherein the Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C.

6. The method of claim 1 , wherein 2 moles of the Group VI element are added to the single phase I-III compound.

7. The method of claim 1 , wherein the Group VI element comprises one of S, Se, and Te.

8. The method of claim 1 , further comprising doping with a Group IV element activator.

9. A method for synthesizing I-III-VI Z compounds, comprising:
melting a Group III element;
subsequently adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound;
subsequently adding a Group VI element to the single phase I-III compound under heat while mixing all constituents; and
growing a bulk crystal from the resulting I-III-VI 2 compound without using a seed crystal.

10. The method of claim 9 , wherein the Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C.

11. The method of claim 9 , wherein 1 mole of the Group I element is added to 1 mole of the Group III element.

12. The method of claim 9 , wherein the Group I element comprises a neutron absorber and the Group III element comprises one of In and Ga.

13. The method of claim 9 , wherein the Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C.

14. The method of claim 9 , wherein 2 moles of the Group VI element are added to the single phase I-III compound.

15. The method of claim 9 , wherein the Group VI element comprises one of S, Se, and Te.

16. The method of claim 9 , further comprising doping with a Group IV element activator.

17. The method of claim 9 , wherein mixing all constituents comprises rotating all constituents at an angle.

Assignees

• Bacock & Wilcox Technical Services Y 12 L L C
• Fisk University
• Cons Nuclear Security Llc

Inventors

• Stowe Ashley
• Burger Arnold

Classifications

• C30B29/46

  Sulfur-, selenium- or tellurium-containing compounds · CPC title

• G01T3/08 Primary

  with semiconductor detectors · CPC title

• G01N23/05

  using neutrons · CPC title

• C30B11/06

  at least one but not all components of the crystal composition being added · CPC title

• C30B11/12 Primary

  Vaporous components, e.g. vapour-liquid-solid-growth · CPC title